US1921773A - Process for the production of zinc sulphate - Google Patents

Description

f atented Aug. 8, 1933 I PROCESS FOR msmo nmmsioszmc SULPHATE i Kurt J. PetschowQPassaic, N. J.) assign'or to.

, Royce Chemical Company, Carlton a Corporation of New Jersey 8 Application December 6, 1930 SerialNo. 500,677 1 No Drawing.

s Claims." ((123-125) My invention relates to the production of zinc sulphate andits separation from impurities and refers particularly to processes for the production of commercial, or chemically pure, zinc sulphate 5.1 from sludges containing zinc salts obtained'from the production of sodium sulphoxylate formaldehyde or of other chemicals.

g In the production of sodium formaldehyde sul-' phoxylate sludges are produced containing large i fjrquantities of zinc salts which are, however so intermixed with other organic and inorganic compounds that it has been found practically impossible to obtain the zinc salts in the form of zinc sulphate in a state of purity which will render it valuable as a commercial product.

This difliculty is especially evident in attempts to produce practically and commercially pure z'inc sulphate from the sludges resulting from the pro-.

duction of sodium formaldehyde sulphoxylate and i i hence these sludges accumulate rapidly as products possessing little or no value.

It is evident that if these sludges can be employed as a raw material for the economic production of soluble zinc sulphate, the cost of the ifisulphoxylate will be reduced and the accumulation of the sludges will be avoided.

Notwithstanding the great variety of undesirable compounds, both organic and inorganic, present in these sludges, I have found it possible to obtain practically all of the zinccompounds in the form of zinc sulphate of such purity as to be practically chemically pure and at a cost of production below the market price of zinc sulphate thus materially reducing the cost of production of- 33 the sulphoxylates. V

The process of my invention accomplishes these desirable results and consists generally, besides the oxides, in converting and destroying thecomplex salts and other salts into their oxides, re-

- moving the soluble compounds, both organicand Inorganic, and converting the zinc compounds into pure zinc sulphate. sodium sulphoxylate formaldehyde, consists mostly of zinc oxide or zinc carbonate with the im- While the quantities of chemicals used in my process naturally vary with the character and contents of the sludge employed, the steps of my -process are in general as followsqv mixture is then filtered.

The zinc sludge from the.

purities which are first already in theused zinc The sludge is brought into a suitable kettle, water is added, heat is applied and made alkaline by'the addition of hydrated lime or ammonia or other suitable alkaline compounds, and air is introduced into the mass under the constant agita-- tion. The insoluble compounds are then separated from the soluble compounds preferably by filtering. This 'step of my process removes partly the soluble compounds and partially Ioxidizes and destroys the complex salts and othersalts. V I Water is then added to the sludge and as'mall amount of acid, preferably sulphuric acid is then added to the sludge and air is blown into the mass during constant agitation and heated. The

sludge is then filtered or decanted and washed with water. ThiS step oxidizes" and destroys practically all of the complex salts to their oxides and removes further soluble compoundswhich may be present.

Water isadded' to the sludge to allo'w formed sulphates to dissolve, sulphuric acidisthenadded to the sludge with thorough agitation, which forms zinc sulphatesolution and the sulphates of other heavy metals if they be present as im-.. purities. I

If there be any heavy metal salts present in, addition to the zinc sulphate, as salts of iron,

the solution is neutralized by means'of calcium carbonate and hydrogen peroxide-is added to convert the ferrous sulphates to ferric sulphates.

Lime and calcium? carbonate callfiuthen added and, stirred. This precipitates, the hydrates of; the heavy metals such as ferric hydrate. The:

I By the' process of m'yinvention; Iproduce practically pure zinc sulphate from sludges of the" character described, a. result that has been pre viously considered impossible, and lean thus convert useless and objectionable sludges into a chemical compound of commercial value.

I do not limit myself to the particular chemicals nor to the particular steps of procedure 'de--@ scribed as these are'given simplyias a means for clearly describing the process of my invention.

What I claim is:--

1. In a process for the production of zinc sulphate solution from sludges containing zinc salts," such as from sludges obtained from the produc tion of sodiumsulphoxylate formaldehyde, the steps which comprise destroying the complex salts, by adding water to the sludge, heating the mass, agitating,'passing air through the mass; thus breaking up the complex salts like zinc sulsoluble products, removing the water soluble compounds like sodium bisulphite, sodium sulphate, treating and dissolving the sludge with sulphuric acid so as to convert the zinc oxide into zinc sulphate and separating the zinc sulphate solution by means of filtering.

2. In a process for the production of zinc sulphate solution from sludges containing zinc salts,

such as from sludges obtained from the production of sodium s'ulphoxylate formaldehyde, the steps which comprise adding water to the sludge, heating the mass with steam, treating the sludge with a current of air, adding a small amount of acid thereto, treating the thus produced mixture with a current of air, removing the water soluble compounds, treating and dissolving the sludge with sulphuric acid, and separating the zinc sulphate solutionby means of filtering.

3. In a process for the production of zinc sulphate solution from sludges containing zinc salts such as from sludges obtained from the production of sodium sulphoxylate formaldehyde, the steps which comprise adding water to the sludge, heating the masswith steam, adding hydrated lime or ammonia, treating the alkaline'sludge with a current of air, removing the water soluble compounds, adding a small amount of acid thereto, treating the thus produced mixture with a current of air, removing the water soluble compounds adding water to the sludge to allow formed sulphates to dissolve, treating and dissolving the sludge with sulphuric acid, and separating the zinc sulphate solution by means of filtering.

4. In a process for the production of zinc'sulphate solution from sludges containing ZlIlC salts,

such as from sludges obtained from the production of sodium sulphoxylate formaldehyde, previously mentioned, the'steps which comprise destroying the complex salts, by adding water to the sludge, heating-the mass with steam, agitating, passing air through the mass thus breaking up the complex salts like zinc sulphoxylate formaldehyde into soluble and insoluble products, removing the water soluble compounds, converting 'the zinc oxide into zinc. sulphate solution by treating anddissolving the sludge with sulphuric acid, neutralize the sludge with calcium carbonate, adding hydrogen peroxide, precipitating the heavy metalswith calcium carbonate and filtering the zinc sulphate solution.

5. In a process for the production of zinc sulphate solution from sludges containing zinc salts, such as from sludges obtained from the produc tion of sodium sulphoxylate' formaldehyde, the

' steps which comprise adding waterto the sludge,

heating the mass with steam, treating the sludge with a current of air, adding a small amount of sulphuric acid, precipitating the heavy metals and separating the zinc sulphate solution by filtration from the precipitating salts of the heavy metals.

6. In a process for the production of zinc sulphate solution from sludges containing zinc salts, such as from sludges obtained from the production of sodium sulphoxylate formaldehyde, the steps which comprise, adding water to the sludge, heating the mass with steam, treating the sludge with a current of air, removing the liquid from the mass, adding 'water'to the sludge and adding a small amount of sulphuric acid, heating, treating said mass with a current of air, filtering and washing the thus produced mass, adding water to the sludge to allow formed sulphates to dissolve, treating and dissolving same with sulphuric acid and filtering the thus formed zinc sulphate solution.

, 7. In a process for the production of zinc sulphate solution from sludges-containing zinc salts, such as from sludges obtained from the production of sodium sulphoxylate formaldehyde, the steps which comprise, adding water to the sludge, treating the mass by means of steam, treating the sludge with a current of air, removing the liquid from the mass, adding water and a small amount of sulphuric acid to the sludge, heating, treating said mass with a current of air, filtering and washing the thus produced mass, adding water to the sludge to allow formed sulphates to dissolve, treating and dissolving same with sulphuric acid, neutralize with calcium carbonate, adding peroxide to the mixture, precipitating the salts of the heavy metals with a solution of a member of the group of salts consisting ing the mixture and crystallizing the zinc sulphate solution from the filtrate.

3. In a process for the production of zinc sulphate solution from sludges containing zinc salts, such as from sludges obtained from the production of sodium sulphoxylate formaldehyde, the steps which comprise, adding water to the sludge, heating the mass wi h steam, adding an alkali, treating the alkaline sludge with a current of air, removing the liquid from the mass, adding a small amount of sulphuric acid, heating with steam, treating said mass with acurrent of air, filtering the thus produced mass and washing it with water, adding water to the sludge to allow fcrrnedsulphates to dissolve, treating and dissolving the sludge with sulphuric acid, neutralizing the zinc sulphate solution with calcium carbonate, adding peroxide to the mixture, precipitating the salts of the heavy metals by adding a solution of a member of the group of salts consisting of calcium carbonate and calcium hydrate, filtering the mixture from the residue and crystallizing the zinc sulphate solution from the filtrate. 7

- KURT J. PETSCHOW.